Effect Temperature On Fluorine Doped Tin Oxide Via Spray ......Effect Temperature On Fluorine Doped Tin Oxide Via Spray Pyrolysis Technique. Agbim, E. Ga, Ikhioya, I. La, b, Agbakwuru

International Journal of Scientific & Engineering Research Volume 10, Issue 6, June-2019 707 ISSN 2229-5518

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Effect Temperature On Fluorine Doped Tin Oxide Via Spray Pyrolysis Technique.

Agbim, E. Ga, Ikhioya, I. La, b, Agbakwuru C. Bc , Oparaku Oc and Ugbaja C. Ma

aDepartment Of Physics And Industrial Physics, Faculty Of Physical Science, Nnamdi Azikiwe University, Awka. b Crystal growth and Material Science Laboratory/Department of Physics and Astronomy, Faculty of Physical Sciences, University of Nigeria, Nsukka, Nigeria cDepartment of Physics/Electronics, Federal Polytechnic, Nekede, Imo State Email: [email protected].

Abstracts.

The synthesis of fluorine doped tin oxide thin films were successfully deposited onto well cleared

glass substrate by varying the deposition temperature. The XRD patterns of the films showed that

the deposited films are polycrystalline in nature having the characteristic peaks of tetragonal

structure of SnO2.The peaks observed are (110), (101), (200), (211) and the preferential growth

along the (110) direction. The current versus voltage plots of the material deposited with 3800C,

3900C and 400oC, which represent sample FT4-FT6 showed a non-linear plot. It was observed to

be non Ohmic semiconducting material. It was also noticed that as the temperature of the

depositing material increases the thickness of the films increases. The resistivity of the material

deposited decreases as the temperature and thickness of the films increases. It was observed that

as the optical absorbance and reflectance decreases the wavelength of the incident radiation

increases and transmittance increases as the wavelength of the incident radiation increases. The

films deposited at 3800C, 3900C and 400oC recorded energy gap of 2.6eV-3.0eV.

Keys words: Spray Pyrolysis, Fluorine, Tin Oxide, XRD and Optical Properties

1. Introduction

Thin films Semiconductor have been studied for many years because of their importance in various

fields like solar cells and gas sensors [1-4]. Transparent conductive oxides of high band gap

semiconductors are mechanically hard and can withstand high temperatures. Also wide and direct

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band gap semiconductor materials are of much interest for blue and ultraviolet (UV) optical

devices, such as light-emitting diodes and laser diodes [5-7]. Tin oxide based thin films are good

candidate for a number of applications in many fields of research and in various optoelectronic

device fabrications [9]. Most important is the thin film application in environmental monitoring

through sensing of a number of gases [10]. Tin oxide characteristics for gas sensing applications

have been improved through catalytic and impurity doping with a view of improving on its

sensitivity to a number of gases as well as its optoelectronic properties [11-12]. Tin oxide based

thin films have been reported to suffer from sensitivity due to the presence of ambient humidity

which has been overcome by resistive heating of the thin film gas sensor element [13]. Tin oxide

is a wide band gap, non-stoichiometric semiconductor material of n-type conductivity. The

conductivity of SnO2 thin films can be manipulated from normal to degenerate by suitably doping

SnO2 with appropriate amount of halogens [11, 14]. Low electrical resistivity and high visible

transmittance are the key elements for solar cell layers, gas sensors, hybrid microelectronics and

opto-electronic devices [15]. SnO2:F coatings can also act as heat mirrors due to their high

reflectivity in the infrared range. Among the various transparent conducting oxides, tin oxide (TO)

films doped with fluorine or antimony are most promising due to their chemical inertness and

mechanical hardness along with low electrical resistivity and good optical transmittance. Tin oxide

is the first transparent conductor to have received significant commercialization [16]. The

application of thin films in modern technology is widespread. The methods employed for thin-film

deposition can be divided into two groups based on the nature of the deposition process viz.,

physical or chemical. The physical methods include physical vapour deposition (PVD), laser

ablation, molecular beam epitaxy, and sputtering. The chemical methods comprise gas-phase

deposition methods and solution techniques. The gas-phase methods are chemical vapour

deposition (CVD) and atomic layer epitaxy (ALE), while spray pyrolysis, sol-gel, spin and dip-

coating methods employ precursor solutions [17]. Among the various deposition techniques, the

spray pyrolysis is well suited for the preparation of doped tin oxide thin films because of its simple

and inexpensive experimental arrangement, ease of adding various doping material,

reproducibility, high growth rate, and mass production capability [16]. Spray pyrolysis is a

processing technique being considered in research to prepare thin and thick films, ceramic

coatings, and powders. Unlike many other film deposition techniques, spray pyrolysis represents

a very simple and relatively cost-effective processing method (especially with regard to equipment

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costs). It offers an extremely easy technique for preparing films of any composition. It does not

require high-quality substrates or chemicals. The method has been employed for the deposition of

dense films, porous films, and for powder production. Even multi layered films can be easily

prepared using this versatile technique. Spray pyrolysis has been used for several decades in the

glass industry and in solar cell production [17]. Typical spray pyrolysis equipment consists of an

atomizer, precursor solution, substrate heater, and temperature controller. The following atomizers

are usually used in spray pyrolysis technique: air blast (the liquid is exposed to a stream of air)

[18], ultrasonic (ultrasonic frequencies produce the short wavelengths necessary for fine

atomization) and electrostatic (the liquid is exposed to a high electric field) [19].

Experimental Details

2.1 Materials And Methods

The various materials were used in the fabrication of the films; Glass substrate, Spray pyrolysis

machine, Ethanol and water as solvent, Precursor SnCl4 (MERCK), Dopant Ammonium fluoride

(BDH), Four-point probe, X-ray diffractometer and UV visible spectrophotometer. Spray

pyrolysis technique was used for this deposition. It involves spraying of a solution containing

soluble salts of the desired compound onto heated substrates, where the constituents react to form

a chemical compound. The chemical reactants used for making solution are selected such that the

products other than the desired compound are volatile at the temperature of deposition. Every

sprayed droplet reaching the surface of the hot substrate undergoes pyrolytic decomposition and

forms a single crystalline or cluster of crystallites as a product. The other volatile by-products and

solvents escape in the vapour phase. The substrates provide thermal energy for the thermal

decomposition and subsequent recombination of the constituent species.

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Figure 1: General schematic of a spray pyrolysis deposition process.

2.2 Substrate (Microscopic Glass Substrate)

The substrate used here is a microscopic glass substrate. Hand gloves were used to handle the

substrates to avoid contamination. The substrates were dipped in acetone, methanol, rinsed with

distilled water and later ultra-sonicated for 30 min in acetone solution after which they were rinsed

in distilled water and kept in an oven at 333K to dry.

2.3 Spray Process/Procedure

The spray process involves optimization of several process parameters. The values of the

optimized process parameters are: Precursor flow rate 0.07ml/min, Solvent 90% ethanol, Precursor

(SnCl4) concentration 0.1mol, Dopant Ammonium Fluoride, Dopant concentration (0.1mol),

Spray-nozzle specification: outside diameter: 0.34mm. Internal diameter 0.18mm, Spray nozzle to

substrate distance: 8mm, Substrate temperature were 3800C, 3900C and 400oC with Atomizing

voltage 3.8KV

2.4 Experimental Procedure

Thin films of fluorine doped thin oxide were deposited on a transparent glass substrate using SnCl4

dissolved in 90ml of ethanol and 10ml of water. The SnCl4 was used as source of Sn while NH4F

as the source of doping impurities. During the deposition, the films were deposited at a constant

dopant concentration and voltage rate of 10% and 3.8KV respectively. The substrate was attached

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to the substrate holder, with the temperature regulator; the substrate was heated to the temperature

at which that particular sample will be deposited. The voltage was set to 3.8KV via the voltage

knob and the precursor solution of SnCl4 and NH4F was passed through the nozzle pump direct to

the nozzle. As the mixture gets to the substrate through the nozzle and hits the surface of the

substrate, evaporation of the residual solvent takes place, spreading of the droplet and then the salt

decomposition SnO2: F was finally deposited on the substrate. Film uniformity was ensured by

moving both the nozzle (needle) and the substrate. Different levels of doping were achieved by

varying the amount of NH4F in the precursor solution from 0.1 to 0.3M. The films with different

level of doping were deposited on the glass substrate at different temperature (see table 1).

Uniformity of temperature over the entire substrate and fine sprays were necessary to obtain good

quality films which are reproducible. The temperature during spray were 3800C, 3900C and 400oC

with the help of the temperature controller whereas the dopant concentration of NH4F was kept

constant (see table 1). After spraying, the substrates were allowed to be cooled at room

temperature.

Table 1: Variations of Temperature Parameters For Fabrication.

Samples Dopant NH4F (%)

SnCl4

(ml)

Ethanol

(ml)

Voltages

(KV)

Temperature

(Degree)

FT4 10 20 5 3.8 380

FT5 10 20 5 3.8 390

FT6 10 20 5 3.8 400

2.5 Characterization Of Fabricated Films.

The fabricated films were characterized using three different instruments for the analysis. The

optical analysis were carried out using MT670 UV- visible spectrophotometer where the

absorbance of each of the samples was obtain and other optical properties were obtained by

calculation. Electrical (I/V) characterization of thin films was done using the four-point probe

method at room temperature. The measurements were taken in a square geometry using Keithley

2400 Source Meter. This was carried out at Sheda Science and Technology Complex, Abuja. The

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structural characterization of the films was carried out using cu-kal (λ = 1.15418Ǻ) DD-15.5

standard diffractometer, the instrument helped in determining the type of crystal lattice and

intensities of diffraction peaks, with the help of data base software supplied by the international

center of diffraction data. The characterization was carried out at IThemba LABS Materials

Research Department South Africa.

Results And Discussion

3.1 Structural Analysis

The XRD analysis was carried out to determine the phase angel, crystallite size and dislocation

density of the films deposited by varing the deposition temperature of the films., deposition

voltage, dopant concentration were kept constant. The XRD patterns of the films prepared by

different deposition parameters showed that the deposited films are polycrystalline in nature

having the characteristic peak of tetragonal crystal structure. The peaks observed are (110), (101),

(200), (211) (see table 2) and among all the peaks the orientation of (110) peak is the highest

intensity peak. This is observed in the patterns of all the films with different deposition parameters

of SnO2:F films prepared from SnCl4 precursor, which also revealed the preferential growth along

the (110) direction. The crystallite sizes of the deposited SnO2:F films were determined from

Scherer’s equation (1) [20].

D = 0.94𝜆𝜆𝛽𝛽𝛽𝛽𝛽𝛽𝛽𝛽𝛽𝛽

(1)

where D is the crystallite size in nanometers, β is the full width at half maximum of the diffraction

line measured in radians and λ is the wavelength of X-ray used (λ= 1.5418Å). The dislocation

density δ is calculated using equation 2 [21-22]. See Figure 2 for the XRD pattern

δ = 1𝐷𝐷2

lines/m2 (2)

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100000 200000 300000 400000 500000 600000 700000 800000 900000-500

0

500

1000

1500

2000

2500

3000

Inte

nsity

(a.u

)

2θ Degree

FT4 3800C FT5 3900C FT6 4000C

110 101200

211

Figure 2: XRD pattern of SnO2:F

Table 2: Structural parameters of fluorine doped tin oxide

Sample/ Thickness

2θ (degree)

d (spacing) Å

(β) FWHM

(hkl) Lattice (a) Å

Grain Size(D) nm

Dislocation density (δ) x1011 lines/m2

FT4/ 10.0087 3.430 0.0642 110 4.7309 18.7721 2.8378 171.229nm 20.0332 3.428 0.0642 101 18.9900 2.7730 30.0543 3.397 0.0642 200 19.3627 2.6673 32.0867 3.378 0.0642 211 19.4584 2.6411

FT5/ 10.0054 3.440 0.0642 110 22.6609 1.9473 171.229nm 19.0756 3.434 0.0642 101 22.8911 1.9084 29.0870 3.321 0.0642 200 23.3231 1.8383 31.0321 3.409 0.0642 211 23.4285 1.8218 FT7/

10.3256 3.294

0.0291

110

50.0067

3.9989

192.609nm 20.2987 3.285 0.0291 101 50.5956 3.9064 30.1943 3.265 0.0291 200 51.5843 3.5515 37.2872 3.243 0.0291 211 52.5620 3.6100

3.2 Electrical Analysis

Electrical characterization of thin films was done using the four-point probe method at room

temperature. The measurements were taken in a square geometry using Keithley2400 Source

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Meter. From (fig. 3 and table 3) the current versus voltage plots of the material deposited with

3800C, 3900C and 400oC, which represent sample FT4-FT6 showed a non-linear plot. It was

observed to be non Ohmic semiconducting material. It was also noticed that as the temperature of

the depositing material increases the thickness of the films increases. The resistivity of the material

deposited decreases as the temperature and thickness of the films increases. The electrical

conductivity of the material deposited increases with respect to the temperature and thickness

respectively [23-24].

Table 3: Calculated values of resistivity and conductivity

Samples Thickness, t (nm)

Resistivity, ρ (Ωm)

Conductivity, σ (Ωm)-1

FT4 (3800C) 171.229 7.4006x106 1.3512x10-7

FT5 (3900C) 174.657 2.0449x105 4.8902x10-6

FT6 (4000C) 178.701 1.0802x105 9.2575x10-6

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Figure 3: Current versus Voltage plot of sample FT74-FT6

3.3 Optical Properties

Optical characterization of the thin films was done using the UV-visible spectrophotometer from

(fig.5) it was observed that as the optical absorbance decreases the wavelength of the incident

radiation increases. It was noticed that sample FT6 deposited at 4000C recorded the highest

absorbance with absorbance value of 0.310 at incident wavelength of 880nm. The sample FT4

deposited at 3800C with absorbance value of 0.234 at incident wavelength of 320nm, hence, it is

very clear that sample FT5 deposited at 3900C recorded absorbance value of 0.244 at incident

wavelength of 420nm. Therefore, the optical absorbance of the deposited material decreases as the

wavelength of the incident radiation increases but has no regular pattern with the temperature

[11,35-40]. From (fig.6) it was observed that as the optical transmittance increases as the

wavelength of the incident radiation increases. It was noticed that sample FT5 deposited at 3900C

emerged the highest transmittance with transmittance value of 0.916% at incident wavelength of

1480nm followed by sample FT4 deposited at 3800C with transmittance value of 0.780% at

incident wavelength of 1480nm. It was observed that sample FT6 deposited at 4000C recorded the

lowest transmittance value of 0.569% at incident wavelength of 1480nm. Therefore, the optical

transmittance of the deposited material increases with the wavelength of the incident radiation [25,

33-37]. From (fig.7). It was noticed that sample FT6 deposited at 400oC emerged the highest

reflectance with reflectance value of 0.200% at incident wavelength of 880nm and stable followed

by sample FT5 deposited at 3900C with reflectance value of 0.186% at incident wavelength of

420nm. Hence, it is very clear that sample FT4 deposited at 3800C emerged the lowest with

reflectance value of 0.182% at incident wavelength of 640nm. Therefore, the optical reflectance

of the deposited material decreases as the temperature of the deposited material (SnO4:F) increases

with the wavelength of the incident radiation [25, 34-38].

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200 400 600 800 1000 1200 1400 16000.00

0.05

0.10

0.15

0.20

0.25

0.30

Abs

orba

nce

(a.u

)

λ (nm)

FT4 3800C FT5 3900C FT6 4000C

Figure 4: The optical absorbance versus wavelength

200 400 600 800 1000 1200 1400 1600

0.5

0.6

0.7

0.8

0.9

1.0

Tran

smitt

ance

(%)

λ (nm)

FT4 3800C FT5 3900C FT6 4000C

Figure 5: The optical transmittance versus wavelength

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200 400 600 800 1000 1200 1400 1600

0.02

0.04

0.06

0.08

0.10

0.12

0.14

0.16

0.18

0.20

Ref

lect

ance

(%)

λ (nm)

FT4 3800C FT5 3900C FT6 4000C

Figure 6: The optical reflectance versus wavelength

The band gap energy of the deposited material was obtained using

𝛼𝛼ℎ𝑣𝑣 = 𝐴𝐴(ℎ𝑣𝑣 − 𝐸𝐸𝑔𝑔)𝑛𝑛

Where 𝐴𝐴 is a constant, 𝐸𝐸𝑔𝑔 is the energy band gap of the material deposited (F: SnO4), ℎ is the

planks constant and𝑛𝑛 = 12 for direct allowed transition. This relation establishes that aplot of

(𝛼𝛼ℎ𝑣𝑣)2versus ℎ𝑣𝑣 produces a linear pattern the intercept on ℎ𝑣𝑣 axis being the energy band gap, 𝐸𝐸𝑔𝑔

of the thin film. The plot is not direct [26, 36-40]. The extrapolations of the direct portions of plots

to the energy axis give the band gap energy. From (fig.7) which represents the material deposited

at 10conc.-30conc. Recorded energy band gap of 2.6eV-3.0eV.

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0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5

0.00E+000

1.00E+011

2.00E+011

3.00E+011

4.00E+011

5.00E+011

6.00E+011

(αhν

)2X1

012 (

eV/c

m)2

hν (eV)

FT4 3800C FT5 3900C FT6 4000C

FT4: 2.6eVFT5: 2.8eVFT6: 3.0eV

Figure 7: The absorption coefficient square versus photon energy FT7

From (Fig. 8), shows that as the optical refractive index value is steady as the photon energy

increases. It was noticed that sample FT6 deposited at 4000C emerged the highest refractive index

with refractive index value of 2.6196 followed by sample FT5 deposited at 3900C with refractive

index value of 2.5154. Hence, sample FT4 deposited at 3800C emerged the lowest with refractive

index value of 2.4870. Therefore, the optical refractive index of the deposited material decreases

as the temperature of the deposited material (SnO4:F) decreases with increase in the photon energy

[11]. From (fig. 9) it was observed that the extinction coefficient maintained a steady value for

sample FT6 and FT4 after a sharp increase and increases for sample FT5 as the photon energy

increases. It was noticed that sample FT6 deposited at 4000C recorded the highest extinction value

of 0.02466, sample FT5 deposited at 3900C with extinction coefficient value of 0.01941 followed

by sample FT4 deposited at 3800C with extinction coefficient value of 0.01881. Hence, the

extinction coefficient of the deposited material increases as the deposition temperature of the

deposited material (SnO4:F) increases with the photon energy [27,36-40]. From (Fig.10) shows

that as the optical conductivity increases with the photon energy. It was noticed that sample FT6

deposited at 4000C emerged the highest with optical conductivity value of 4.3716E+13 followed

by sample FT5 deposited at 3900C with optical conductivity value of 4.0555E+13 and sample FT4

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deposited at 3800C recorded optical conductivity value of 4.0453E+13 Hence, the optical

conductivity of the deposited material increases as the temperature of the deposited material

(SnO4:F) increases with the photon energy [11,28-35].

0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5

1.4

1.6

1.8

2.0

2.2

2.4

2.6

Ref

ract

ive

inde

x (n

)

hν (eV)

FT4 3800C FT5 3900C FT6 4000C

Figure 8: The refractive index versus photon energy

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0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.50.000

0.005

0.010

0.015

0.020

0.025

Extin

ctio

n co

effic

ient

(k)

hν (eV)

FT4 3800C FT5 3900C FT6 4000C

Figure 9: The extinction coefficient versus photon energy

0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5

0.00E+000

1.00E+013

2.00E+013

3.00E+013

4.00E+013

5.00E+013

Opt

ical

con

duct

ivity

(S-1

)

hν (eV)

FT4 3800C FT5 3900C FT6 4000C

Figure 10: The optical conductivity versus photon energy

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Conclusion

Fluorine doped tin oxide thin films have been successfully deposited and characterized at different deposition parameters. The absorbance, reflectance decreases and transmittance of the films increases as the wavelength of the films increases with incident radiation. It was observed that as the voltage of the films increases the thickness of the films increases. The conductivity of the films was observed to be increasing with decrease in voltage.

Acknowledgement The authors are grateful to the staff of iThemba Laboratory of Materials Research Department South Africa, the staff of energy centre, ABU-Zaria, and finally Kaduna Polytechnic Centre for Minerals Research & Development Science and Technology Education Post-basic (Step-B) Project (World Bank Assisted) were the characterization was done.

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